Manufacture of improved asphalt



- M y 14 1940. RE. MK 5+ AL 2.200.914

MANUFACTURE OF IMPROVED ASPHALT Filed July 14, 1938 ,Blowzlrzg at 500 500 :1? 4

asphalt Patented May 14, 1940 UNITED STATES MANUFACTURE or IMPROVED ASPHALT Robert E. Burk and Charles H. Whitacre, Cleveland, Ohio, assignors to The Standard Oil Com,-

pany, Cleveland, Ohio, :1. corporationol' Ohio Application July 14, 1938, Serial No. 219,186

5 Claims.

ing of hydrocarbon molecules. It has not been possible though to attain products with melting point as'high as are desirable for a given penetration. In accordance with the present invention however,asphalts of remarkably high melting point for a given penetration may be produced, such products having particular value in usageswhere exposed to sun and air.

To the accomplishment of the foregoing and related ends, the invention. then, comprises the features hereinafter fully described, and particularly pointed out in the claims, the following description setting forth in detail certain illus- 25 trative embodiments of the invention, these beingindicative however, of but a few of the various ways in which the principle of the invention may be employed.

The accompanying drawing is aflow sheet illus- 30 trating diagrammatically a preferred embodiment of the invention.

In our co-pending application Ser. No. 219,405,

filed July 15, 1938, there is set forth the making of asphalt by air-blowing residuum and 'subse- 35 quently treating with a hydro-halogen acid and a halide. In the present process; first the stock to be worked up, a heavy hydrocarbon material containing aliphatic hydrocarbons, for instance a petroleum oil residue. and which-we designate 40 residuum, and which with particular advantage may be in some instances a mixture of .pipe still bottoms and cylinder oil stock, the latter for example in proportion of to 30 per cent, is heated with oxygen or air, conveniently for'instance be- 45 ing blown with air. The temperature of treatment may be 225-450 F., the material being suitably stirred or agitated. And the tim:- of this treatment may be for instance 12 to 24 hours. With the ,air or at least during the latter portion of the air-blowing there is carried into the .material, most conveniently with the air current, a small amount of chlorine. Having in this manner brought the up to partial specification, the air-b fwing is discontinued, likewise.

f, the atalytic chlorine Then. while maintaining commercial procedure, by air-blowing to finished -'by. the present invention, and for comparable .But, if the residuum be air-blown and catalytic the temperature elevated, for instance at 300-450 a. small amount of aluminum chloride,AlCla,

is incorporated into the residuum, and is allowed to act for 15 to 60 minutes. The amount of aluminum chloride may be 0.1 to 1.0 per cent, 5 usually 0.25 per cent. In some cases we also add a small amount of a hydro-halogen acid, as a hydrogen chloride, (H01). hydrogen bromide, (HBr), hydrogen fluoride, (HF) hydrogen iodide, HI), in general the number of mols of hydro- 10 halogen acid not exceeding the number of molsv ofthe halogen catalyst.

Products produced in accordance withthe present procedure are asphalts of extraordinarily high melting point with relation to the penetration. 15 These products also have outstanding susceptibility cocfflcients and have great resistance to oxidation, and are capable of particularly excellent performance in usages such as roofing asphalt, paving filler asphalts, etc., where subjected to-partlcularly drastic exposure to sun and oxidation action. That the action in the present process is not merely the additive efiects of oxidation with catalysts and then treatment with aluminum chloride. is shown from'comparative tests. Thus, a residuum treated in accordance with customary specification, shows a melting point of 219, withv penetration 18 at 77 and 31 at 115. If the same residuum be blown with air and catalytic chlorine. the product comes out with a melting point M219", and penetration 13 at 77 and 26 at 115".

If similar residuum be treated I with aluminum chloride alone in the small amount contemplated time, the product comes out with a melting point of 222, and penetration 20 at 77 and 3'7 at 115.

chlorine be supplied, and then the air-blowing be discontinued, and 0.25 per cent of aluminum chloride be incorporated in accordance with the present invention, the product comes out for instance with a melting point of 241 and penetration 11 at 77 and 20 at 115. Melting point relations heretofore unobtainable thus become possible.

This application is a continuation, in part an as to common subject matter, of our application Ser. No. 112.848, filed November 23, 1938.

Other modes ofapplying the principle of the invention may be employed, change being made as regards the details described, provided the features stated in any of the following claims, I

,or the equivalent of such,.be employed.

tinuing the aforesaid and introducing into the residuum a small amount of aluminum chloride anda small amount of a hydro-halogen acid and subjecting the residuum to the action thereof at elevated temperature.

3. A process of making asphalt, which com- 0 prises air-blowing a residuum and introducing a small amount of chlorine, then discontinuing the air-blowing and introducing into the residuum 0.25 per cent of aluminum chloride and maintaining the temperature elevated.

4. A process of making asphalt, which comprises oxidizing a residuum and introducing a small amount of chlorine during at least the latter part of the oxidizing action, then discontinuing the aforesaid and introducing into the residuum a small amount of aluminum chloride and subjecting the residuum to the action thereof at elevated temperature.

5. A process of making asphalt, which comprises air-blowing a residuum and introducing a small amount of chlorine, then discontinuing the air-blowing and introducing into the residuum a v small amount of aluminum chloride and maintaining the temperature elevated.

ROBERT E. BURK.

CHARLES H. WHITACRE. 

